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Outgassing data, derived from tests at 396 K (125 C) for 24 hours in vacuum as per ASTM E 595-77, have been compiled for numerous materials for spacecraft use. The data presented are the total mass loss (TML) and the collected volatile condensable materials (CVCM). The various materials are compiled by likely usage and alphabetically.
Dual Sorbent Tubes (DSTs) are currently the primary method for collecting volatile organic compounds in the cabin air of the International Space Station (ISS). Data from groundbased analysis of these archival air samplers provide a major component of the assessment of ISS air quality by the NASA toxicologist. At the 2005 ICES conference data from the positive control DSTs, returned on Soyuz 7S and 8S, were presented. Positive control tubes are dosed, preflight, with known concentrations of representative contaminant compounds and they are launched to ISS in the DST kit as trip controls. Upon return of the DST kit to the ground, results from analysis of the trip (positive) and laboratory control tubes are used to determine the recoveries: concentration of dosed compounds retained in the tube. Results from positive controls, returned on 7S and 8S showed substantial losses of some compounds dosed into the tubes 156 to 240 days prior to the analysis. Low recoveries are expected for spacecraft air contaminants with similar properties to the poorly recovered dosed compounds. It was shown that compound losses in the control tubes were consistent, which led to the generation of acceptable correction factors for spacecraft air contaminants. Correction factors decrease the accuracy of derived compound concentrations and substantial error could arise under some conditions. An investigation into the mechanism for compound loss is necessary before design modifications can be implemented to improve the DST performance. This paper will update results from the DSTs returned on Soyuz 9S and 10S missions during the latter part of 2005. The data acquired from these returned DSTs will be compared to the 7S and 8S data presented last year. Discussion will focus on the reliability of correction factors and identify any trends in the data. This paper will describe the experimental design and plans to identify the compound loss mechanism.
A universal docking and berthing system is being developed by the National Aeronautics and Space Administration (NASA) to support all future space exploration missions to low-Earth orbit (LEO), to the Moon, and to Mars. The Low Impact Docking System (LIDS) is being designed to operate using a seal-on-seal configuration in numerous space environments, each having unique exposures to temperature, solar radiation, reactive elements, debris, and mission duration. As the LIDS seal is likely to be manufactured from an elastomeric material, performance evaluation of elastomers after exposure to atomic oxygen (AO) and ultraviolet radiation (UV) was conducted, of which the work presented herein was a part. Each of the three candidate silicone elastomer compounds investigated, including Esterline ELA-SA-401, and Parker Hannifin S0383-70 and S0899-50, was characterized as a low outgassing compound, per ASTM E595, having percent total mass loss (TML) less than 1.0 percent and collected volatile condensable materials (CVCM) less than 0.1 percent. Each compound was compatible with the LIDS operating environment of -50 to 50 C. The seal characteristics presented include compression set, elastomer-to-elastomer adhesion, and o-ring leakage rate. The ELA-SA-401 compound had the lowest variation in compression set with temperature. The S0383-70 compound exhibited the lowest compression set after exposure to AO and UV. The adhesion for all of the compounds was significantly reduced after exposure to AO and was further decreased after exposure to AO and UV. The leakage rates of o-ring specimens showed modest increases after exposure to AO. The leakage rates after exposure to AO and UV were increased by factors of up to 600 when compared to specimens in the as-received condition.
Outgassing data, derived from tests at 398 K (125 C) for 24 hours in vacuum as per ASTM E-595-90, have been compiled for numerous materials designed for spacecraft use. The data presented are the total mass loss (TML) and the collected volatile condensable materials (CVCM). The various materials are compiled by likely usage, and then in alphabetical order.
Radiation blocking sunscreen coatings have been developed for the protection of elastomer seals used in low-Earth-orbit (LEO). The coatings protect the seals from ultraviolet (UV) radiation and atomic oxygen (AO) damage. The coatings were developed for use on NASA docking seals. Docking seal damage from the UV and AO present in LEO can constrain mission time-line, flight mode options, and increases risk. A low level of adhesion is also required for docking seals so undocking push-off forces can be low. The coatings presented also mitigate this unwanted adhesion. Greases with low collected volatile condensable materials (CVCM) and low total mass loss (TML) were mixed with slippery and/or UV blocking powders to create the protective coatings. Coatings were applied at rates up to 2 milligrams per square centimeter. Coated seals were exposed to AO and UV in the NUV (near-UV) and UV-C wavelength ranges (300 to 400 nanometers and 254 nanometers, respectively). Ground based ashers were used to simulate the AO of space. The Sun's UV energy was mimicked assuming a nose forward flight mode, resulting in an exposure rate of 2.5 megajoules per square meter per day. Exposures between 0 and 147 megajoules per square meter (UV-C) and 245 megajoules per square meter (NUV) were accomplished. The protective coatings were durable, providing protection from UV after a simulated docking and undocking cycle. The level of protection begins to decline at coverage rates less than 0.9 milligrams per square centimeter. The leakage of seals coated with Braycote plus 20 percent Z-cote ZnO sunscreen increased by a factor of 40 after moderate AO exposure; indicating that this coating might not be suitable due to AO intolerance. Seals coated with DC-7-16.4 percent Z-cote ZnO sunscreen were not significantly affected by combined doses of 2 x 10 (sup 21) atoms per square AO with 73 megajoules per square meter UV-C. Unprotected seals were significantly damaged at UV-C exposures of 0.3 megajoules per square meter and DC-7-16.4 percent Z-cote coated seals were undamaged at all exposures up to the limits tested thus far which were 147 megajoules per square meter UV-C and 245 megajoules per square meter NUV. The coatings decreased adhesion sufficiently for docking seals at temperatures equal to or greater than -8 degrees Centigrade thus offer a simple and inexpensive way to mitigate adhesion.
Skills Acquired: Tensile Testing: Prepare materials and setting up the tensile tests; Collect and interpret (messy) data. Outgassing Testing: Understand TML (Total Mass Loss) and CVCM (Collected Volatile Condensable Material); Collaboration with other NASA centers. Z2 (NASA's Prototype Space Suit Development) Support: Hands on building mockups of components; Analyze data; Work with others, understanding what both parties need in order to make a run successful. LCVG (Liquid Cooling and Ventilation Garment) Flush and Purge Console: Both formal design and design review process; How to determine which components to use - flow calculations, pressure ratings, size, etc.; Hazard Analysis; How to make design tradeoffs.
The capability of the gas capture cell to collect particles and semivolatile species which were released during impact is examined. The proposed Comet Coma Sample Return (CCSR) payload contains a variety of instrumentation for characterizing and collecting cometary dust. In this suite of instruments the Gas Capture Cell (GCC) is unique in that it not only collects the vaporization products resulting from the dust particle impacts, but also provides chemical characterization information prior to return of the dust particles for analysis on Earth. The GCC provides near real-time characterization of the volatile species, such as low- and medium-molecular-weight organic compounds that evolve from dust particles on impact with metal targets. Instrument sensitivity is sufficient for analyzing the volatile impact products resulting from single, individual dust particles. This capability will enable characterization of near-pristine dust particles, including the CHON particles, to be performed at a level not previously possible. Its design concept, operation and performance are detailed.
A device for the extraction and collection of volatiles from soil or planetary regolith. The device utilizes core drilled holes to gain access to underlying volatiles below the surface. Microwave energy beamed into the holes penetrates through the soil or regolith to heat it, and thereby produces vapor by sublimation. The device confines and transports volatiles to a cold trap for collection.
A system and methodology were developed for the nondestructive qualitative and quantitative analysis of volatile emissions from hydroponically grown 'Waldmann's Green' leaf lettuce (Lactuca sativa L.). Photosynthetic photon flux (PPF), photoperiod, and temperature were automatically controlled and monitored in a growth chamber modified for the collection of plant volatiles. The lipoxygenase pathway products (Z)-3-hexenal, (Z)-3-hexenol, and (Z)-3-hexenyl acetate were emitted by lettuce plants after the transition from the light period to the dark period. The volatile collection system developed in this study enabled measurements of volatiles emitted by intact plants, from planting to harvest, under controlled environmental conditions.
Current arts to create linear motion or acceleration of fine particles and molecules into devices such as mass spectrometers and vacuum pumps rely on the pressure difference created by a pinhole or mechanical processes. However, in an environment of vacuum, these approaches do not create such a pressure differential to drive and move fine particles and molecules. In some cases, electrostatic or magnetic processes may work to create the desired motion. A cylindrical harmonic of electric field, which is widely used in electron accelerators, offers a unique capability to capture and induce a linear motion of molecules and particles when electrically charged. Generally, lunar volatiles are electrostatically charged. The idea to capture and collect the lunar volatiles by creating a drift axis of motion using a cylindrical harmonic field has led to the development of a device concept, called a Bessel Tube. The Bessel Tube concept ingests fine particles, gaseous atoms, and gaseous molecules and guides them along an extraction tube for collection, separation, and analysis. The Bessel Tube concept for lunar volatile collection is discussed.
To sustain affordable human and robotic space exploration, the ability to live off the land at the exploration site will be essential. NASA calls this ability in situ resource utilization (ISRU) and is focusing on finding ways to sustain missions first on the Moon and then on Mars. The ISRU project aims to develop capabilities to technology readiness level 6 for the Robotic Lunar Exploration Program and early human missions returning to the Moon. NASA is concentrating on three primary areas of ISRU: (1) excavating, handling, and moving lunar regolith, (2) extracting oxygen from lunar regolith, and (3) finding, characterizing, extracting, separating, and storing volatile lunar resources, especially in the permanently shadowed polar craters. To meet the challenges related to technology development for these three primary focus areas, the Regolith and Environment Science and Oxygen and Lunar Volatile Extraction (RESOLVE) project was initiated in February 2005, through funding by the Exploration Systems Mission Directorate. RESOLVE's objectives are to develop requirements and conceptual designs and to perform breadboard concept verification testing of each experiment module. The final goal is to deliver a flight prototype unit that has been tested in a relevant lunar polar environment. Here we report progress toward the third primary area creating ways to find, characterize, extract, separate, and store volatile lunar resources. The tasks include studying thermal, chemical, and electrical ways to collect such volatile resources as hydrogen, water, nitrogen, methane, and ammonia. We approached this effort through two subtasks: lunar water resource demonstration (LWRD) and regolith volatile characterization (RVC).
Lunar Flashlight is an exciting new mission concept in preformulation studies for NASA's Advanced Exploration Systems (AES) by a team from the Jet Propulsion Laboratory, UCLA, and Marshall Space Flight Center. This innovative, low-cost concept will map the lunar south pole for volatiles and demonstrate several technological firsts, including being the first CubeSat to reach the Moon, the first mission to use an 80 m2 solar sail, and the first mission to use a solar sail as a reflector for science observations. The Lunar Flashlight mission spacecraft maneuvers to its lunar polar orbit and uses its solar sail as a mirror to reflect 50 kW of sunlight down into shaded polar regions, while the on-board spectrometer measures surface reflection and composition. The Lunar Flashlight 6U spacecraft has heritage elements from multiple cubesat systems. The deployable solar sail/reflector is based on previous solar sail experiments, scaled up for this mission. The mission will demonstrate a path where 6U CubeSats could, at dramatically lower cost than previously thought possible, explore, locate and estimate size and composition of ice deposits on the Moon. Locating ice deposits in the Moon's permanently shadowed craters addresses one of NASA's Strategic Knowledge Gaps (SKGs) to detect composition, quantity, distribution, form of water/H species and other volatiles associated with lunar cold traps. Polar volatile data collected by Lunar Flashlight could then ensure that targets for more expensive lander- and rover-borne measurements would include volatiles in sufficient quantity and near enough to the surface to be operationally useful.
Freon-113(TradeMark) has been used as a chemistry lab sampling solvent at NASA/JSC for EMU (extravehicular Mobility Unit) SOP (Secondary Oxygen Pack) oxygen testing Cold Traps utilized at the USA (United Space Alliance) Houston facility. Similar testing has occurred at the HSWL (Hamilton Sundstrand Windsor Locks) facility. A NASA Executive Order bans the procurement of all ODS (ozone depleting substances), including Freon-113 by the end of 2009. In order to comply with NASA direction, HSWL began evaluating viable solvents to replace Freon-113 . The study and testing effort to find Freon-113 replacements used for Cold Trap sampling is the subject of this paper. Test results have shown HFE-7100 (a 3M fluorinated ether) to be an adequate replacement for Freon-113 as a solvent to remove and measure the non-volatile residue collected in a Cold Trap during oxygen testing. Furthermore, S-316 (a Horiba Instruments Inc. high molecular weight, non-ODS chlorofluorocarbon) was found to be an adequate replacement for Freon-113 as a solvent to reconstitute non-volatile residue removed from a Cold Trap during oxygen testing for subsequent HC (hydrocarbon) analysis via FTIR (Fourier Transform Infrared Spectroscopy).
The Volatile Organics Concentrator (VOC) system, designed to attach to a gas chromatograph/mass spectrometer (GC/MS) for the analyses of volatile organic compounds in water on Space Station Freedom, is described. Organic volatiles are collected and concentrated in the VOC by means of two primary solid sorbent tubes and desorbed into the GC/MS system. The paper describes the results of testing the VOC breadboard using a GC/MS system. Evaluations performed on 39 organic compounds recovered from water samples were compared with data for these compounds using direct injection/GC/MS and purge and trap/GC/MS procedures. The results demonstrate that the VOC/GC/MS system's detection limits for the 39 compounds analyzed are comparable to those of the EPA Method 524.2, and for many compounds reaching a factor of 5 lower.
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Various investigators propose the lunar surface contains widely distributed volatiles, especially water- like species, i.e. OH and H2O. Surface volatiles are theorized to exist as a hydrated regolith layer, concentrated in extremely cold polar permanently shadowed regions (PSR), and/or solar wind implantation reservoirs in lunar glasses. The proposed sources of lunar surface volatiles range from cometary impacts, solar wind, or a supply present during moon formation. Future Artemis missions aim to collect and return the samples containing volatiles collected near lunar polar craters or PSRs. We, as advanced curation scientists, are responsible for developing techniques and methodologies for preserving returned sample integrity as much as possible. Pristine volatile-bearing samples are invaluable to the scientific community seeking to unravel the history of the solar system. Realistically, a sample will experience alteration during collection, transportation back to earth, and storage. The Planetary Exploration and Astromaterials Research Lab (PEARL) seeks to understand temperature and pressure effects on high-fidelity volatile-containing regolith simulants, the foundation for the future of cold curation. This abstract outlines the separation, identification, and quantification of headspace gases over volatile ice feed stock material using gas chromatography/mass spectrometry (GC/MS). Preliminary objectives concentrated on sample handling, reproducibility, and understanding the elution characteristics for each analyte. Initial GC/MS method development experiments utilized diluted static headspace sample preparation. Diluted samples were used because sampling headspace gases directly from a vial containing liquid analyte resulted in overloading of the column and detector. Overloading is evident based on chromatogram peak shapes and instrument contamination, or carry over, between experiments. A mixture of three alcohols were used for a majority of the sample handling and reproducibility studies. Reproducibility was tested via multiple users, calibration curves, and check standards. Stock solutions of condensed lunar volatile analytes included methanol, ammonia in methanol, hydrogen sulfide in water, and an equal volume mixture of methanol, ethanol, and isopropanol. Current samples use room air as the headspace sample matrix, however future experiments will incorporate an inert purge gas, such as argon or nitrogen. Three mL of each analyte solution were capped in separate 20 mL crimp top GC vials. Dilutions were carried out by removing an aliquot of headspace gases with a calibrated 1 mL gastight syringe and immediately transferring to a 20 mL capped crimp top vial. The GC/MS is a Thermo Fisher Trace 1310/ISQ 7000 with a TriPlus RSH autosampler and split/splitless injector module. The experiments outlined in this abstract use the following hardware: a 2.5 mL gastight headspace syringe tool, 1 mm ID x 78.5 mm length ultra-inert straight injection liner, and a TG-BondQ 30 m × 0.32 mm × 10 μm column. Various parameters, such as hardware selection and the temperature, pressure, and split ratio set points, continue to evolve as the overall experiment is refined. Diluted headspace chromatograms were collected for the individual stock solutions. Retention times, peak shapes, and mass spectra were evaluated and added to the data processing method for each molecule of interest. Figure 1 shows the total ion chromatograms for the three major lunar volatile simulant stock solutions: methanol, 7 N ammonia in methanol, and 0.4% hydrogen sulfide in water. Tailing peak shapes for ammonia (2.98 min rt) and water (4.06 min rt) indicate the molecules are not properly eluting from the selected column with the current separation method. Additionally, hydrogen sulfide and ammonia have overlapping peak windows, which could impact quantification. Ongoing experiments aim to address the peak shape and overlapping via the separation method and hardware selection. Sample preparation reproducibility experiments used stock solution containing equal volumes of a non- interactive mixture of methanol, ethanol, and isopropanol. Mass spectrum ion traces were used to identify and quantify all three alcohols. Peaks were automatically detected, identified, and integrated through the mass spectra detection and processing parameters. Calibration response curves and check standards were used to evaluate the validity of the sample preparation procedure. Figure 2 shows the methanol chromatogram peak area versus total headspace dilution volume transferred from the alcohol mixture vial. The calibration response curves and check standards validate sample preparation procedure. Continuing data analysis efforts are working towards correlating the peak area and instrument response factor to the headspace analyte concentration and condensed phase composition. Static headspace gas chromatography theory relies on Dalton’s law, Raoult’s law, Henry’s Law, and the Kolb and Ettre equation to associate peak area to the analyte composition in a non-ideal solution. Equation 1 is a simplified expression derived from the aforementioned theories. Future experiments involve liquid injections of the individual stock solutions, liquid and headspace analysis of various stock solution combinations, and the addition of regolith simulants to the mixtures. Temperature is another variable expected to affect reaction rates and will be explored.
One of the major questions remaining for the future exploration of the Moon by humans concerns the presence of volatiles on our nearest neighbor in space. Observational studies, and investigations involving returned lunar samples and using robotic spacecraft infer the existence of volatile compounds particularly water [1]. It seems very likely that a volatile component will be concentrated at the poles in circumstances where low-temperatures exist to provide cryogenic traps. However, the full inventory of species, their concentration and their origin and sources are unknown. Of particular importance is whether abundances are sufficient to act as a resource of consumables for future lunar expeditions especially if a long-term base involving humans is to be established. To address some of these issues requires a lander designed specifically for operation at a high-lunar latitude. A vital part of the payload needs to be a volatile analyzer such as the Gas Analysis Package specifically designed for identification quantification of volatile substances and collecting information which will allow the origin of these volatiles to be identified [1]. The equipment included, particularly the gas analyzer, must be capable of operation in the extreme environmental conditions to be encountered. No accurate information yet exists regarding volatile concentration even for sites closer to the lunar equator (because of contamination). In this respect it will be important to understand (and thus limit) contamination of the lunar surface by extraneous material contributed from a variety of sources. The only data for the concentrations of volatiles at the poles comes from orbiting spacecraft and whilst the levels at high latitudes may be greater than at the equator, the volatile analyzer package under consideration will be designed to operate at the highest specifications possible and in a way that does not compromise the data.
Introduction: Future Artemis missions aim to return the volatile-bearing samples collected near lunar polar craters. We, as advanced curation scientists, are responsible for developing techniques and methodologies for preserving the integrity of returned samples and the science value those samples contain. The extent to which that preservation is possible, and the trade-offs preservation requires (e.g. monetary costs, sample volume limitations) all must be considered. Even less-than pristine volatile-bearing samples will be of tremendous value to the scientific community seeking to unravel the history of lunar surface volatiles and, more broadly, volatiles in the solar system. A sample collected on the lunar surface will experience at least five distinctive periods during which any changes here referred to as “alteration” will certainly occur at some scale: collection on the lunar surface; transportation back to Earth; long-term storage; curatorial processing; and allocation/distribution. The Planetary Exploration and Astromaterials Research Lab (PEARL) seeks to understand temperature and pressure effects on returned volatile samples by working with high-fidelity volatile-containing regolith simulants, setting the foundation for the future of cold curation. This abstract is focused on gas-surface interactions between LCROSS volatiles and readily available lunar regolith simulants. Experiments involved analyzing differences in headspace gas composition for various combinations of volatile and regolith simulants using gas chromatography/mass spectrometry (GC/MS). Experimental Procedure: The volatile simulants were chosen based on the molecules detected during the LCROSS mission.1 Stock solutions of condensed lunar volatile analytes were: methanol, 7 N ammonia in methanol, and 0.4% hydrogen sulfide in water. The regolith simulants used were primarily JSC-1A and NU-LHT-4M. Additional regolith simulant control studies were conducted with <150 μm sieved sand and KBr. A nested vial sample preparation approach separated the liquid stock solutions from the regolith, eliminating potential matrix effects between liquid and solid phases. Fifteen microliter aliquots of liquid volatile simulants were added to a 2 mL liquid GC vial and capped in atmosphere. An 18G needle punctured the 2 mL GC vial immediately before being transferred and sealed in a 20 mL GC vial containing 0-0.3 g of regolith simulant, see Figure 1. Separating the analytes ensures any changes observed in the total headspace gases is a result of gas-surface and/or gas-gas interactions. Equipment and Method: Initial GC/MS method development for the separation and identification of relevant headspace gases can be found in Amick, et al. 2023.2 The only hardware change is a different column: a TG-1701MS 30 m × 0.25 mm × 1.00 μm column. The vials were sampled at 10°C, room temperature (~25°C) and 50°C. Low temperature samples were kept in a chilled autosampler stage for at least 1 hour prior to sampling. High temperature samples were agitated at 50°C for 5 minutes immediately prior to injection onto the column. Headspace chromatograms were collected for each combination of temperature, regolith, and volatile simulant, including controls without one or both types of analytes, in triplicate. The chromatogram elution window for each analyte or significant atmospheric gas was identified using the peak mass spectrum cross-referenced with Figure 1.Picture of the nested vial set-up. a NIST MS library search. Each analyte peak was integrated after filtering the mass spectrum trace for the parent or most unique mass-to-charge ratio. For example, the mass-to-charge ratio used to identify, filter for, and integrate the carbon dioxide peak was centered around 44 m/z. Results: Figure 2 shows the integrated peak area for hydrogen sulfide in all combinations of regolith simulants, temperatures, and the addition of ammonia in methanol solution. Multiple repeat experiments with H2S and regolith simulants have confirmed hydrogen sulfide is removed from the headspace within 1 hour when exposed to JSC-1A, NU-LHT-4M and sand (not pictured). The consumption of H2S by lunar regolith simulants at different temperatures indicates surface chemistry will be an integral component in sample integrity and preservation. It is important to note that while the effect of surface chemistry on gaseous hydrogen sulfide is intriguing, further investigation into more chemically accurate regolith simulants is necessary and ongoing. The sulfur in hydrogen sulfide is in its most reduced state while off-the-shelf, terrestrially sourced JSC-1A and NU-LHT-4M are more oxidized than most lunar materials,3which likely leads to different oxidation-reduction reactions than would be expected in lunar regolith. Figure 3 shows the integrated peak area of carbon dioxide for each sample combination that contained ammonia in methanol solution. The addition of ammonia to the GC vials results in a consistent and reproducible decrease in carbon dioxide gas, even at 50°C. The effect became more pronounced when JSC-1A or NU-LHT-4M were present. This set of experiments demonstrated that the sample composition will affect the chemical and physical state of each component present. Future spectroscopic and microscopy experiments will be geared towards identifying the cause for the CO2(g) concentration decrease and the consumption of hydrogen sulfide. As cold and volatile curation scientists, this information provides necessary insight on how to appropriately handle and analyze volatile bearing returned samples, as well as predict the effect chemical composition has on the various sample phases we will analyze upon return to Earth. Unlike traditional curation of geologic materials, the molecules in a sample cannot be identified or processed using the naked eye or even an optical microscope. Volatile curation will require a combination of analytical techniques, including but not limited to highly sensitive gas and solid/condensed phase spectroscopy. This set of experiments has demonstrated the need for more detailed studies of volatile mixtures with mineralogically and geochemically analogous lunar regolith simulants to prepare for the curation of volatile-rich lunar samples from the south polar region of the Moon. References: [1] Colaprete, A., et al. (2010) Science, 330, (463-468). [2] Amick, C. L., et al.(2023) Houston, Texas, [3] Heiken, G. H., et al.(1991) (778-778)